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An air-assisted dispersive micro solid phase extraction method (AA-dμ-SPE) is described that is based on the use of a magnetic graphitic carbon nitride (g-C₃N₄/Fe₃O₄) nanocomposite. In AA-dμ-SPE, magnetic nanocomposite was dispersed into the aqueous sample solution by air bubbles, which promoted the analytes adsorption. The magnetic adsorbents were then separated from sample solution using a magnetic field. The method was shown to be efficient, rapid and reliable to extract the polycyclic aromatic hydrocarbons (PAHs) from biological samples prior to their determination by GC with FID detection. The nanocomposite was characterized by X-ray diffraction, FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometer and thermogravimetric techniques. A main reason of selection of the g-C₃N₄/Fe₃O₄ nanocomposites as adsorbent is their …